CN108892516A - A kind of ceramic membrane compression moulding preparation method and its product obtained - Google Patents
A kind of ceramic membrane compression moulding preparation method and its product obtained Download PDFInfo
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- CN108892516A CN108892516A CN201810847698.9A CN201810847698A CN108892516A CN 108892516 A CN108892516 A CN 108892516A CN 201810847698 A CN201810847698 A CN 201810847698A CN 108892516 A CN108892516 A CN 108892516A
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Abstract
The invention discloses a kind of ceramic membrane compression moulding preparation methods, the flat ceramic film support with several raised lines is prepared using dry pressing first, then intermediate layer and teleblem or only one layer of teleblem are prepared on ceramic film support, later by the way of being glued encapsulation, by forming infiltration lane between raised line, so that asymmetric ceramic membrane be made.Product made from above-mentioned compression moulding preparation method is utilized in addition, also disclosing.Preparation method simple process of the present invention, low in cost, operating condition is easily-controllable, high production efficiency, the problems such as efficiently solving easily-deformable prior art membrane, complex process, it not only facilitates and improves product quality and application, and large scale ceramic membrane can be prepared;Obtained ceramic membrane product High anti bending strength, separating property are excellent, can be widely applied to the separation fields such as solid-liquid, liquid-liquid.The present invention is versatile, is conducive to industrialized mass production, application market has a extensive future.
Description
Technical field
The present invention relates to the preparation method of ceramic membrane materials technical field more particularly to a kind of ceramic membrane and its it is made
Product.
Background technique
Ceramic membrane is the important component of high performance membrane material, because having high temperature resistant, resistance to chemical attack, mechanical strength
Well, the advantages that anti-microbe ability is strong, permeation flux is big, clanability is strong, pore-size distribution is narrow, long service life, in medicine, stone
Numerous industrial circles such as oil and chemical industry, food, environmental protection, metallurgy have been widely used, it has also become film field is developed most
Rapidly, most one of the membrane material of application prospect.
Classify according to ceramic membrane structure and production technology characteristic, ceramic membrane can be divided into tubular ceramic membrane and flat ceramic
Two kinds of film.Ceramic membrane belongs to low-pressure membrane, therefore more more energy efficient than tubular ceramic membrane, and ceramic membrane has structure letter
It is single, separative efficiency is high, easy to operate, composability is strong, many advantages such as easy to clean, to be obtained in water process Practical Project
It must be widely applied, and achieve good operational effect.
Currently, the main preparation methods of prior art ceramic membrane include:Extrusion moulding, doctor-blade casting process, gel
Casting, sol-gel method etc..Although above-mentioned preparation method is applied in a certain range, but still generally existing
The technological deficiencies such as membrane is easily-deformable, technique is more complex, equipment requirement is high, operation is more complex, high expensive, greatly hinder
The further genralrlization and development of flat ceramic film preparation and application.Especially, currently as general in flat ceramic membrane preparation technology
All over the extrusion moulding used, membrane is dry and sintering process in, it is especially prominent that membrane deforms big problem, not only serious shadow
Product quality and application have been rung, and has caused diaphragm plate specification limited, has been not easy to prepare large scale ceramic membrane (at present
The full-size of conventional panel ceramic membrane product is long 1m × wide 50cm).Therefore, it needs to research and develop new ceramic membrane system
Standby technology, to effectively facilitate the further development of flat ceramic film preparation and application.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of simple processes, low in cost, operating condition
Easily-controllable, high production efficiency asymmetric ceramic membrane compression moulding preparation method is had using dry pressing preparation several first
The flat ceramic film support of raised line obtains asymmetric ceramic membrane, then by film firing, in conjunction with assembling with effective
The problems such as solving easily-deformable prior art membrane, complex process.Another object of the present invention is to provide made pottery using above-mentioned plate
Product made from porcelain film compression moulding preparation method.
The purpose of the present invention is achieved by the following technical programs:
A kind of ceramic membrane compression moulding preparation method provided by the invention, includes the following steps:
(1) using big particle size ceramic powder as raw material, it is the water of 3~8wt% of ceramic powder, 0.5~1wt% that dosage, which is added,
The pore creating material of binder, 0~5wt% after being mixed, is aging, being granulated, using dry pressuring forming process, obtains having the flat of raised line
Plate shaped ceramic supporter;The raised line is distributed in the lower surface of ceramic film support, consistent with supporter length direction and be in
Spacing parallel arranging arrangement;
(2) slurry is prepared as film-coating material, in the upper table of the ceramic film support by raw material of small particle ceramic powder
Wheat flour obtains the asymmetric ceramic membrane element of tabular through drying, firing for teleblem or transition zone and teleblem;
(3) two asymmetric ceramic membrane elements are connected to each other with raised line and carry out splicing encapsulation, obtained asymmetric flat
Plate ceramic membrane.
The present invention uses dry pressing to prepare the flat ceramic film support with several raised lines first, then in ceramic membrane
Intermediate layer and teleblem or only one layer of teleblem are prepared on supporter, later by the way of being glued encapsulation, by shape between raised line
At infiltration lane, so that asymmetric ceramic membrane be made.
Further, in step (1) of the present invention the used ceramic powder of ceramic film support average grain diameter be 5~
50μm;Transition zone in the step (2), the used ceramic powder of teleblem average grain diameter be respectively 2~10 μm, 0.1~1 μm.
In above scheme, according to the ceramic powder of unlike material, using firing or not firing process.Ceramics of the present invention
Powder is aluminium oxide, titanium oxide, cordierite, zirconium oxide, after dry-pressing formed in the step (1), in 1300~1680 DEG C of temperature
Lower firing obtains the tabular ceramic film support with raised line.Alternatively, the ceramic powder be silicon carbide, clayey, it is described
In step (1) it is dry-pressing formed after to get to raised line tabular ceramic film support.The binder be concentration be 5~
The poly-vinyl alcohol solution or cmc soln of 10wt%;The pore creating material is starch or carbon dust.
In addition, the polyvinyl alcohol that water is added by small particle ceramic powder in film-coating material of the present invention and concentration is 10wt%
Solution mixed preparing forms, wherein prepares water in the film-coating material of transition zone, the dosage of poly-vinyl alcohol solution is respectively small particle pottery
50~70wt%, the 20~40wt% of ceramic powder.
Further, the pressure of its dry-pressing of step (1) of the present invention is 20~50MPa;Dry temperature in the step (2)
Degree is 40~80 DEG C, and firing temperature is 1100~1450 DEG C.
In above scheme, ceramic film support of the present invention with a thickness of 1~5mm, the height of the raised line is 0.5~
2mm, bottom width are 0.5~3mm;The transition zone with a thickness of 10~50 μm;The teleblem with a thickness of 10~50 μm.Institute
State the height of raised line: raised line spacing=1: 1~6.
For convenient for shaping and demoulding, its cross section of raised line of the present invention is inverted trapezoidal (bevel edge angle is 30~80 °),
It can be rectangular, semicircle etc.;Binding site on the external edge edge of ceramic film support and raised line and supporter has down
Angle, can be radian is π/6~5 π/6 arc-shaped.
Utilize product made from above-mentioned ceramic membrane compression moulding preparation method.
The invention has the advantages that:
(1) present invention prepares flat ceramic film support using dry pressing, efficiently solves the prior art using crowded
The technologies such as the generally existing membrane of the methods of molding is easily-deformable out, complex process, equipment requirement are high, complicated for operation, at high cost
Problem, has many advantages, such as to be simple and efficient, low in cost, operating condition is easily-controllable, versatile, easy to spread, be conducive to industrialize
Batch production, application market have a extensive future.
(2) the present invention is based on dry pressings to be prepared, and membrane deformation is small, not only facilitates and improves product quality and answer
With, and there is technical advantage in the size for prepare ceramic membrane, it solves the problems, such as that diaphragm plate specification is limited, can make
Standby length out is greater than 1000mm, width is greater than the ceramic membrane product of 500mm.
(3) preparation method of the present invention obtains ceramic membrane product High anti bending strength, separating property are excellent, and (its anti-folding is strong
Degree is 40~65MPa, pure water permeation flux is 1200~2620Lm-2·h-1·bar-1), it can be widely applied to solid-liquid, liquid-
The separation fields such as liquid.
Detailed description of the invention
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail:
Fig. 1 is the preparation technology flow chart of ceramic membrane compression moulding preparation method embodiment of the present invention;
Fig. 2 is the assembling schematic diagram of ceramic membrane element in ceramic membrane compression moulding preparation method embodiment of the present invention.
Specific embodiment
Embodiment one:
A kind of ceramic membrane compression moulding preparation method of the present embodiment, as shown in Figure 1, its step are as follows:
(1) alumina powder for being 50 μm using average grain diameter is added in an amount of alumina powder 8wt%'s as raw material
The poly-vinyl alcohol solution (concentration 5wt%) of water, 0.5wt%, after being mixed, be aging, being granulated, in the case where pressure is 50MPa, compacting
Out having a size of long 300 × wide by 100 × thickness 1mm, external edge along the tabular ceramic film support base in arc-shaped (radian is π/3)
Body, lower surface are evenly equipped with the raised line consistent with supporter length direction, in spacing parallel arranging arrangement that 39 height are 0.5mm
(its cross section of raised line is as shown in Figure 2 a in inverted trapezoidal, and trapezoidal hypotenuse angle is 30 °, bottom width 0.5mm, raised line
Chamfering radian with supporter binding site is π/3);After 1680 DEG C of firings, tabular ceramic film support is obtained;
(2) alumina powder for being 10 μm using average grain diameter is added in an amount of alumina powder 50wt%'s as raw material
Poly-vinyl alcohol solution (concentration 10wt%) preparation of water, 40wt% obtains slurry as transition zone film-coating material, using dip coating,
And after 40 DEG C of dry 3h, the transition zone with a thickness of 20 μm is prepared in the upper surface of above-mentioned ceramic film support;
The alumina powder for being 1 μm using average grain diameter as raw material, be added in an amount of alumina powder 60wt% water,
Poly-vinyl alcohol solution (concentration 10wt%) preparation of 30wt% obtains slurry as teleblem film-coating material, using spray coating method, upper
It states to prepare on transition zone and, in 1450 DEG C of firing 1h, it is non-right to obtain tabular after 80 DEG C of dry 0.5h with a thickness of 20 μm of teleblem
Claim ceramic membrane element;
(3) as shown in Figure 2 a, two above-mentioned asymmetric ceramic membrane elements are connected to each other with raised line and carry out splicing encapsulation, that is, made
Obtain asymmetric ceramic membrane.
The flexural strength of the asymmetric ceramic membrane of the present embodiment is 43MPa, pure water permeation flux is 2504Lm-2·h-1·bar-1。
Embodiment two:
A kind of ceramic membrane compression moulding preparation method of the present embodiment, as shown in Figure 1, its step are as follows:
(1) cordierite powder for being 5 μm using average grain diameter is raw material, be added in an amount of cordierite powder 6wt% water,
The cmc soln (concentration 10wt%) of the starch of 5wt%, 0.5wt%, after being mixed, is aging, being granulated, in pressure
Under 40MPa, suppress having a size of long 600 × wide by 200 × thickness 1mm, external edge along the tabular in arc-shaped (radian is 2 π/3)
Ceramic film support green body, lower surface be evenly equipped with 49 height be 1mm it is consistent with supporter length direction, be in spacing parallel arranging
(its cross section of raised line is as shown in Figure 2 a in inverted trapezoidal to the raised line of arrangement, and trapezoidal hypotenuse angle is 60 °, and bottom width is
The chamfering radian of 1mm, raised line and supporter binding site is 2 π/3);After 1350 DEG C of firings, the support of tabular ceramic membrane is obtained
Body;
(2) cordierite powder for being 0.2 μm using average grain diameter is added in an amount of cordierite powder 60wt%'s as raw material
Poly-vinyl alcohol solution (concentration 10wt%) preparation of water, 30wt% obtains slurry as teleblem film-coating material, using spray coating method,
The upper surface preparation of above-mentioned ceramic film support, in 1150 DEG C of firing 2h, obtains after 40 DEG C of dry 1h with a thickness of 30 μm of teleblem
To the asymmetric ceramic membrane element of tabular;
(3) as shown in Figure 2 a, two above-mentioned asymmetric ceramic membrane elements are connected to each other with raised line and carry out splicing encapsulation, that is, made
Obtain asymmetric ceramic membrane.
The flexural strength of the asymmetric ceramic membrane of the present embodiment is 51MPa, pure water permeation flux is 1860Lm-2·h-1·bar-1。
Embodiment three:
A kind of ceramic membrane compression moulding preparation method of the present embodiment, as shown in Figure 1, its step are as follows:
(1) silicon carbide powder for being 5 μm using average grain diameter is raw material, be added in an amount of silicon carbide powder 3wt% water,
The poly-vinyl alcohol solution (concentration 10wt%) of the carbon dust of 5wt%, 1wt%, after being mixed, is aging, being granulated, in pressure 20MPa
Under, it suppresses having a size of long 600 × wide by 100 × thickness 2mm, external edge along the tabular ceramic membrane in arc-shaped (radian is π/3)
Supporter, lower surface are evenly equipped with the raised line consistent with supporter length direction, in spacing parallel arranging arrangement that 24 height are 2mm
(its cross section of raised line is rectangular, bottom width 1mm as shown in Figure 2 b, the chamfering radian of raised line and supporter binding site
For π/6);
(2) silicon carbide powder for being 2 μm using average grain diameter is added in an amount of silicon carbide powder 70wt%'s as raw material
Poly-vinyl alcohol solution (concentration 10wt%) preparation of water, 20wt% obtains slurry as transition zone film-coating material, using dip coating,
And through 80 DEG C of dry 2h, the transition zone with a thickness of 20 μm is prepared in the upper surface of above-mentioned ceramic film support;
The silicon carbide powder for being 0.1 μm using average grain diameter as raw material, be added in an amount of silicon carbide powder 60wt% water,
Poly-vinyl alcohol solution (concentration 10wt%) preparation of 30wt% obtains slurry as teleblem film-coating material, using leaching slurry processes, upper
It states to prepare on transition zone and, in 1180 DEG C of firing 1h, it is non-right to obtain tabular after 80 DEG C of dry 0.5h with a thickness of 20 μm of teleblem
Claim ceramic membrane element;
(3) as shown in Figure 2 b, two above-mentioned asymmetric ceramic membrane elements are connected to each other with raised line and carry out splicing encapsulation, that is, made
Obtain asymmetric ceramic membrane.
The flexural strength of the asymmetric ceramic membrane of the present embodiment is 49MPa, pure water permeation flux is 1288Lm-2·h-1·bar-1。
Example IV:
A kind of ceramic membrane compression moulding preparation method of the present embodiment, as shown in Figure 1, its step are as follows:
(1) Zirconium powder for being 10 μm using average grain diameter is added in an amount of Zirconium powder 8wt%'s as raw material
The cmc soln (concentration 5wt%) of water, 0.5wt%, after being mixed, be aging, being granulated, at pressure 40MPa, pressure
It produces having a size of long 300 × wide by 100 × thickness 1mm, external edge along the tabular ceramic film support in arc-shaped (radian is π/6)
Green body, lower surface are evenly equipped with the raised line consistent with supporter length direction, in spacing parallel arranging arrangement that 24 height are 1mm
(its cross section of raised line is semicircle as shown in Figure 2 c, bottom width 1mm, the chamfering arc of raised line and supporter binding site
Degree is 2 π/3);After 1480 DEG C of firings, tabular ceramic film support is obtained;
(2) Zirconium powder for being 3 μm using average grain diameter is added in an amount of Zirconium powder 60wt%'s as raw material
Poly-vinyl alcohol solution (concentration 10wt%) preparation of water, 30wt% obtains slurry as transition zone film-coating material, using dip coating,
And through 60 DEG C of dry 1.5h, the transition zone with a thickness of 30 μm is prepared in the upper surface of above-mentioned ceramic film support;
The Zirconium powder for being 0.5 μm using average grain diameter as raw material, be added in an amount of Zirconium powder 60wt% water,
Poly-vinyl alcohol solution (concentration 10wt%) preparation of 30wt% obtains slurry as teleblem film-coating material, using spray coating method, upper
It states to prepare on transition zone and, in 1250 DEG C of firing 2h, it is non-right to obtain tabular after 80 DEG C of dry 0.5h with a thickness of 15 μm of teleblem
Claim ceramic membrane element;
(3) as shown in Figure 2 c, two above-mentioned asymmetric ceramic membrane elements are connected to each other with raised line and carry out splicing encapsulation, that is, made
Obtain asymmetric ceramic membrane.
The flexural strength of the asymmetric ceramic membrane of the present embodiment is 65MPa, pure water permeation flux is 2148Lm-2·h-1·bar-1。
Embodiment five:
A kind of ceramic membrane compression moulding preparation method of the present embodiment, as shown in Figure 1, its step are as follows:
(1) titanium oxide powder for being 30 μm using average grain diameter is added in an amount of titanium oxide powder 6wt%'s as raw material
Water, the starch of 5wt%, 1wt% poly-vinyl alcohol solution (concentration 10wt%), through mix, it is aging, be granulated after, in pressure
Under 50MPa, suppress having a size of long 600 × wide by 200 × thickness 1mm, external edge along the tabular in arc-shaped (radian is 5 π/6)
Ceramic film support green body, lower surface be evenly equipped with 39 height be 1mm it is consistent with supporter length direction, be in spacing parallel arranging
(its cross section of raised line is rectangular, bottom width 1.5mm as shown in Figure 2 b, raised line and supporter engaging portion to the raised line of arrangement
The chamfering radian of position is 5 π/6);After 1300 DEG C of firings, tabular ceramic film support is obtained;
(2) titanium oxide powder for being 5 μm using average grain diameter is added in an amount of titanium oxide powder 60wt%'s as raw material
Poly-vinyl alcohol solution (concentration 10wt%) preparation of water, 30wt% obtains slurry as transition zone film-coating material, using drenching slurry processes,
And through 70 DEG C of dry 1h, the transition zone with a thickness of 30 μm is prepared in the upper surface of above-mentioned ceramic film support;
The titanium oxide powder for being 1 μm using average grain diameter as raw material, be added in an amount of titanium oxide powder 60wt% water,
Poly-vinyl alcohol solution (concentration 10wt%) preparation of 30wt% obtains slurry as teleblem film-coating material, using dip coating, upper
It states to prepare on transition zone and, in 1100 DEG C of firing 1h, it is non-right to obtain tabular after 80 DEG C of dry 0.5h with a thickness of 15 μm of teleblem
Claim ceramic membrane element;
(3) as shown in Figure 2 b, two above-mentioned asymmetric ceramic membrane elements are connected to each other with raised line and carry out splicing encapsulation, that is, made
Obtain asymmetric ceramic membrane.
The flexural strength of the asymmetric ceramic membrane of the present embodiment is 50MPa, pure water permeation flux is 2603Lm-2·h-1·bar-1。
Embodiment six:
A kind of ceramic membrane compression moulding preparation method of the present embodiment, as shown in Figure 1, its step are as follows:
(1) alumina powder for being 50 μm using average grain diameter is added in an amount of alumina powder 8wt%'s as raw material
The poly-vinyl alcohol solution (concentration 5wt%) of water, 0.5wt%, after being mixed, be aging, being granulated, in the case where pressure is 50MPa, compacting
Out having a size of long 1200 × wide by 600 × thickness 2mm, external edge along the tabular ceramic film support in arc-shaped (radian is π/3)
Green body, lower surface are evenly equipped with the raised line consistent with supporter length direction, in spacing parallel arranging arrangement that 49 height are 2mm
(its cross section of raised line is as shown in Figure 2 a in inverted trapezoidal, and trapezoidal hypotenuse angle is 60 °, bottom width 3mm, raised line with
The chamfering radian of supporter binding site is π/3);After 1680 DEG C of firings, tabular ceramic film support is obtained;
(2) alumina powder for being 10 μm using average grain diameter is added in an amount of alumina powder 50wt%'s as raw material
Poly-vinyl alcohol solution (concentration 10wt%) preparation of water, 40wt% obtains slurry as transition zone film-coating material, using dip coating,
And after 40 DEG C of dry 3h, the transition zone with a thickness of 25 μm is prepared in the upper surface of above-mentioned ceramic film support;
The alumina powder for being 1 μm using average grain diameter as raw material, be added in an amount of alumina powder 60wt% water,
Poly-vinyl alcohol solution (concentration 10wt%) preparation of 30wt% obtains slurry as teleblem film-coating material, using spray coating method, upper
It states to prepare on transition zone and, in 1450 DEG C of firing 1h, it is non-right to obtain tabular after 80 DEG C of dry 0.5h with a thickness of 20 μm of teleblem
Claim ceramic membrane element;
(3) as shown in Figure 2 a, two above-mentioned asymmetric ceramic membrane elements are connected to each other with raised line and carry out splicing encapsulation, that is, made
Obtain asymmetric ceramic membrane.
The flexural strength of the asymmetric ceramic membrane of the present embodiment is 41MPa, pure water permeation flux is 2516Lm-2·h-1·bar-1。
Claims (10)
1. a kind of ceramic membrane compression moulding preparation method, it is characterised in that include the following steps:
(1) using big particle size ceramic powder as raw material, it is the water of 3~8wt% of ceramic powder, 0.5~1wt% bonding that dosage, which is added,
Agent, 0~5wt% pore creating material, through mix, it is aging, be granulated after, using dry pressuring forming process, obtain the tabular with raised line
Ceramic film support;The raised line is distributed in the lower surface of ceramic film support, it is consistent with supporter length direction and in interval
Arranged in parallel;
(2) slurry is prepared as film-coating material, in the upper surface system of the ceramic film support by raw material of small particle ceramic powder
Standby teleblem or transition zone and teleblem, through drying, are burnt into, obtain the asymmetric ceramic membrane element of tabular;
(3) two asymmetric ceramic membrane elements are connected to each other with raised line and carry out splicing encapsulation, obtain asymmetric plate pottery
Porcelain film.
2. ceramic membrane compression moulding preparation method according to claim 1, it is characterised in that:In the step (1)
The average grain diameter of the used ceramic powder of ceramic film support is 5~50 μm;Transition zone, teleblem are used in the step (2)
The average grain diameter of ceramic powder is respectively 2~10 μm, 0.1~1 μm.
3. ceramic membrane compression moulding preparation method according to claim 1, it is characterised in that:The ceramic powder is
Aluminium oxide, titanium oxide, cordierite, zirconium oxide are burnt at a temperature of 1300~1680 DEG C after dry-pressing formed in the step (1),
Obtain the tabular ceramic film support with raised line.
4. ceramic membrane compression moulding preparation method according to claim 1, it is characterised in that:The ceramic powder is
Silicon carbide, clayey, it is dry-pressing formed in the step (1) after to get to the tabular ceramic film support with raised line.
5. ceramic membrane compression moulding preparation method according to claim 1 or 2 or 3 or 4, it is characterised in that:It is described
Binder is the poly-vinyl alcohol solution or cmc soln that concentration is 5~10wt%;The pore creating material is starch or carbon
Powder.
6. ceramic membrane compression moulding preparation method according to claim 1, it is characterised in that:The step (1) its
The pressure of dry-pressing is 20~50MPa;Drying temperature is 40~80 DEG C in the step (2), and firing temperature is 1100~1450 DEG C.
7. ceramic membrane compression moulding preparation method according to claim 1, it is characterised in that:The ceramic membrane support
Body with a thickness of 1~5mm, the height of the raised line is 0.5~2mm, bottom width is 0.5~3mm;The thickness of the transition zone
It is 10~50 μm;The teleblem with a thickness of 10~50 μm.
8. ceramic membrane compression moulding preparation method according to claim 1 or claim 7, it is characterised in that:The raised line
Highly: raised line spacing=1: 1~6.
9. ceramic membrane compression moulding preparation method according to claim 1 or claim 7, it is characterised in that:The raised line with
The binding site of supporter is chamfering setting;Its cross section of the raised line is inverted trapezoidal or rectangular, semicircle.
10. utilizing product made from ceramic membrane compression moulding preparation method described in one of claim 1-9.
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